CN103213991A - Recovery and cyclic utilization technology for electronic-level waste acid mixture - Google Patents
Recovery and cyclic utilization technology for electronic-level waste acid mixture Download PDFInfo
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- CN103213991A CN103213991A CN2013101545576A CN201310154557A CN103213991A CN 103213991 A CN103213991 A CN 103213991A CN 2013101545576 A CN2013101545576 A CN 2013101545576A CN 201310154557 A CN201310154557 A CN 201310154557A CN 103213991 A CN103213991 A CN 103213991A
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Abstract
The invention relates to a recovery and cyclic utilization technology for an electronic-level waste acid mixture. The recovery and cyclic utilization technology is used for adding and analyzing sodium salt or potassium salt solid to form fluosilicate solid precipitate according to the content of fluosilicic acid in the acid mixture under a compulsory stirring condition by adopting high-concentration nitric acid, hydrofluoric acid and fluosilicic acid liquid waste which are generated in a wool making process of the electronic industry, as the materials; the precipitate is filtered and dried for sale in the form of high-purity fluosilicate; and the mother solution is directly used for a recycling line. The recovery and cyclic utilization technology has the characteristics of being simple in process thought, environmentally-friendly, efficient and the like.
Description
Technical field
The present invention relates to a kind of electronic-grade mixing spent acid and reclaim and recycle utilization, belong to electron trade changing rejected material to useful resource comprehensive reutilization field.
Background technology
Along with the exhaustion of earth fossil energy, sun power, wind energy, Geothermal energy, the utilization of tidal energy equal energy source progressively become the main mode that people's energy obtains.Solar electrical energy generation is the main mode that sun power utilizes.And silica-based solar cell is one of mature technology of current solar electrical energy generation.The solar electrical energy generation process is environmental protection, but is highly energy-consuming in the preparation process of solar cell, high pollution.China becomes solar energy production base the biggest in the world, and the maximum pollution in the world is also being carried in China simultaneously.For the oneself, for the descendants, we must take necessary action to administer pollution problem.The every square polycrystal silicon cell sheet making herbs into wool of 156mm needs 7ml nitric acid, 10ml hydrofluoric acid.Every the production of polysilicon line can produce several tons high density making herbs into wool spent acid every day.These spent acid can only be handled to give up admittedly.Serious environmental issues such as nitrogen discharged, fluorine discharging have been caused.
Hydrofluoric acid such as fluorite prepare raw material and belong to Nonrenewable resources.Rose in 2010, country has put into effect the relevant policy measure and has limited its outlet.The recycling of fluoride waste also is a kind of protection to non-renewable data such as fluorites.Country and district government have put into effect the policy of recycling economy accordingly.Also be to protect and keeping Sustainable development.
Adopt sodium hydroxide, potassium hydroxide making herbs into wool in the solar energy single crystal making herbs into wool.Residual aspects such as efficient to sun power through follow-up cleaning sodium, potassium do not have a significant impact.Adopt the processing mode of adding sodium salt, sylvite that the sun power manufacturing processed is not had considerable influence.Characteristics such as solar energy polycrystal making herbs into wool has the concentration height with nitration mixture, and complicated component, metals content impurity are extremely low.If with conventional unslaked lime solidification treatment, a large amount of solid useless and wastings of resources will be produced.If after the silicofluoric acid separation, stoste can be got back to and be produced line continuation use.Silicofluoride after the separation can directly be sold with the form of high purity reagent.This will produce great benefit.
Find through the document investigation, aspect the recycling of electron trade waste liquid.Only Japan three closes oiling and can accomplish the taking back and process of TFT etching with phosphoric acid.Aspect the recycling of sun power making herbs into wool nitration mixture, because the leather producing process difference that each sun power manufacturer uses, the composition difference of the spent acid of making herbs into wool, the difficulty of comprehensive recycling is bigger, currently also is in the blank stage.
To sum up, though also be in the blank stage about the recycling application facet of high density hydrofluoric acid containing, nitric acid, silicofluoric acid waste liquid.But its recycling has huge economic benefit and social benefit.
Summary of the invention
Technical problem to be solved by this invention is the recycling at the high pollution of current sun power industry, excessive risk, high-concentration waste liquid, is a kind of method of complete innoxious use.
For solving the problems of the technologies described above, the present invention takes following technical scheme:
A kind of electronic-grade mixing spent acid reclaims and recycle utilization, comprises the following steps of carrying out successively:
(1), analyzes the mass concentration of nitric acid, hydrofluoric acid, silicofluoric acid in the waste liquid;
(2), under stirring condition, add solid sodium salt or sylvite in the waste liquid of step (1), the mol ratio of described sodium salt or sylvite and silicofluoric acid is 0.9 ~ 2:1;
(3), step (2) gained reaction solution is left standstill 0.5 ~ 2h;
(4), the reaction solution after will leaving standstill filters;
(5), the mass concentration of nitric acid, hydrofluoric acid in the reaction solution after the analysis and filter, and interpolation electronic-grade salpeter solution or hydrofluoric acid solution, the mass concentration of nitric acid is adjusted into 15 % ~ 20%, the mass concentration of hydrofluoric acid is adjusted into 5 % ~ 10 %, the mass concentration of silicofluoric acid is adjusted into less than 5 %, then adjusted reaction solution is sent back to production line and uses;
(6), silicofluoride crystal washing that filtration is obtained, behind 100 ~ 150 ℃ of oven dry 2 ~ 3h, obtain the silicofluoride product then.
Particularly, the mass concentration of nitric acid is that the mass concentration of 5 % ~ 20%, hydrofluoric acid is that the mass concentration of 3% ~ 15 %, silicofluoric acid is 8 % ~ 30 % in the described waste liquid.
Particularly, the total acidity of described waste liquid is greater than 50%.
Particularly, in the described waste liquid metallic cation concentration except that sodium ion, potassium ion less than 1ppm.Therefore, in entire operation, to guarantee the totally pollution-free of sour contact components such as pipeline.
Particularly, in the step (2), churning time is 1 ~ 3h.
Particularly, described sodium salt or sylvite are selected from any in analytically pure saltpetre, SODIUMNITRATE, Potassium monofluoride, Sodium Fluoride, salt of wormwood, the yellow soda ash.
Particularly, the described sodium salt more than the 90wt% or the salt granularity of sylvite can be passed through 40 mesh sieves.
The control of the control of churning time and salt granularity is in order to guarantee the abundant dissolving of sylvite or sodium salt.
Particularly, in the step (4), the reaction solution after leaving standstill is adopted 0.5 micron filter element filtering earlier, then filtrate is adopted 0.01 micron filter element filtering again.Adopt twice filtration to be because if directly adopt the less filter core in aperture to filter, can cause filtration efficiency to hang down inferior problem.
Particularly, the purity of described silicofluoride product is greater than 99%.
Because the enforcement of above technical scheme, the present invention compared with prior art has following advantage:
The present invention is a raw material with polycrystalline making herbs into wool high density spent acid, the high density silicofluoric acid in the Separation and Recovery spent acid, and silicofluoric acid is converted into high-purity silicofluoride product, the reaction solution after the separation returns production line fully and uses; Thereby the high density spent acid complete resource that polycrystalline making herbs into wool produces utilizes, and technological line is reasonable in design ingenious, invests lowly, and benefit is big.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described in detail, but the invention is not restricted to following examples.
Embodiment 1
Get certain making herbs into wool spent acid 200kg of unit, HF content 5.921wt% wherein, HNO
3
Content 16.461wt%, H
2
SIF
6
Content 18.436wt%.Total acidity is 51.25wt%; Metallic cation concentration except that sodium ion, potassium ion is less than 1ppm.
Calculate and take by weighing required analytically pure KNO
3
49.39kg.KNO more than 90%
3
The salt granularity can pass through 40 mesh sieves.
Under stirring condition, slowly in mixing solutions, add saltpetre.
Stir after 1 hour, reaction is finished, and has crystalline deposit to produce.
Reaction solution after leaving standstill is adopted 0.5 micron filter element filtering earlier, then filtrate is adopted 0.01 micron filter element filtering again.
The dry white powder that gets, drying is 2 hours under 120 ℃ of conditions of baking oven, the 51.37kg(that weighs disregards filtration, transfer indfficiency), deserved in theory 53.80kg, net yield 95.5%.
The Sodium Silicofluoride purity testing, purity〉99.4%.
Filtered liquid after the filtration is measured its each component concentration, records HF content 5.851%, HNO
3
Content 32.551%, H
2
SIF
6
Content is less than 0.5% nitration mixture etching solution 198kg.
Embodiment 2
Get certain making herbs into wool spent acid 200kg of unit, wherein HF content 7.025%, HNO
3
Content 18.696%, H
2
SIF
6
Content 14.953%.Total acidity is 53.91wt%; Metallic cation concentration except that sodium ion, potassium ion is less than 1ppm.
Calculate and take by weighing required analytically pure Na
2
CO
3
21.13kg.Na more than 90%
2
CO
3
The salt granularity can pass through 40 mesh sieves.
Under stirring condition, slowly in mixing solutions, add yellow soda ash.
Stir after 1 hour, reaction is finished, and has crystalline deposit to produce.
Reaction solution after leaving standstill is adopted 0.5 micron filter element filtering earlier, then filtrate is adopted 0.01 micron filter element filtering again.
The dry white powder that gets, drying is 2 hours under 120 ℃ of conditions of baking oven, the 35.98kg(that weighs disregards filtration, transfer indfficiency), deserved in theory 37.48kg, net yield 96.0%.
The Sodium Silicofluoride purity testing, purity〉99.3%.
Filtered liquid after the filtration is measured its each component concentration, records HF content 7.001%, HNO
3
Content 14.553%, H
2
SIF
6
Content is less than 0.5%.Add 1.1kg71% nitric acid, get HF content 6.953%, HNO
3
Content 15.102%, H
2
SIF
6
Content is less than 0.5% nitration mixture etching solution 174kg.
Embodiment 3
Get certain making herbs into wool spent acid 200kg of unit, wherein HF content 6.117%, HNO
3
Content 13.677%, H
2
SIF
6
Content 20.641%; Total acidity is 51.00wt%; Metallic cation concentration except that sodium ion, potassium ion is less than 1ppm.
Calculate and take by weighing required analytically pure solid Na
2
CO
3
28.869kg.Na more than 90%
2
CO
3
The salt granularity can pass through 40 mesh sieves.
Under stirring condition, slowly in mixing solutions, add yellow soda ash.
Stir after 1 hour, reaction is finished, and has crystalline deposit to produce.
Reaction solution after leaving standstill is adopted 0.5 micron filter element filtering earlier, then filtrate is adopted 0.01 micron filter element filtering again.
The dry white powder that gets, drying is 2 hours under 120 ℃ of conditions of baking oven, the 48.64kg(that weighs disregards filtration, transfer indfficiency), deserved in theory 51.20kg, net yield 95.0%.
The Sodium Silicofluoride purity testing, purity〉99.3%.
Filtered liquid after the filtration is measured its each component concentration, records HF content 6.005%, HNO
3
Content 11.650%, H
2
SIF
6
Content is less than 0.5%.Add 8.01kg71% nitric acid make HF content 5.682%, HNO
3
Content 15.061%, H
2
SIF
6
Content is less than 0.5% nitration mixture etching solution 170kg.
Embodiment 4
Get certain making herbs into wool spent acid 200kg of unit, wherein HF content 7.423%, HNO
3
Content 12.132%, H
2
SIF
6
Content 20.030%, total acidity are 53.04wt%; Metallic cation concentration except that sodium ion, potassium ion is less than 1ppm.
Calculate and take by weighing required analytically pure solid Na
2
CO
3
27.866kg.Na more than 90%
2
CO
3
The salt granularity can pass through 40 mesh sieves.
Under stirring condition, slowly in mixing solutions, add yellow soda ash.
Stir after 1 hour, reaction is finished, and has crystalline deposit to produce.
Reaction solution after leaving standstill is adopted 0.5 micron filter element filtering earlier, then filtrate is adopted 0.01 micron filter element filtering again.
The dry white powder that gets, drying is 2 hours under 120 ℃ of conditions of baking oven, the 46.705kg(that weighs disregards filtration, transfer indfficiency), deserved in theory 49.42kg, net yield 94.5%.
The Sodium Silicofluoride purity testing, purity〉99.5%.
Filtered liquid after the filtration is measured its each component concentration, records HF content 7.321%, HNO
3
Content 11.652%, H
2
SIF
6
Content is less than 0.5%.Add 8.01kg71% nitric acid make HF content 5.835%, HNO
3
Content 15.101%, H
2
SIF
6
Content is less than 0.5% nitration mixture etching solution 170kg.
Embodiment 5
Get certain making herbs into wool spent acid 200kg of unit, wherein HF content 5.531%, HNO
3
Content 14.876%, H
2
SIF
6
Content 19.584%, total acidity are 50.01wt%; Metallic cation concentration except that sodium ion, potassium ion is less than 1ppm.
Calculate and take by weighing required analytically pure solid Na
2
CO
3
27.62kg.Na more than 90%
2
CO
3
The salt granularity can pass through 40 mesh sieves.
Under stirring condition, slowly in mixing solutions, add yellow soda ash.
Stir after 1 hour, reaction is finished, and has crystalline deposit to produce.
Reaction solution after leaving standstill is adopted 0.5 micron filter element filtering earlier, then filtrate is adopted 0.01 micron filter element filtering again.
The dry white powder that gets, drying is 2 hours under 120 ℃ of conditions of baking oven, the 46.93kg(that weighs disregards filtration, transfer indfficiency), deserved in theory 48.98kg, net yield 95.8%.
The Sodium Silicofluoride purity testing, purity〉99.1%.
Filtered liquid after the filtration is measured its each component concentration, records HF content 5.412%, HNO
3
Content 13.14%, H
2
SIF
6
Content is less than 0.5%.Add 4.01kg71% nitric acid make HF content 5.245%, HNO
3
Content 15.052%, H
2
SIF
6
Content is less than 0.5% nitration mixture etching solution 170kg.
More than the present invention has been done detailed description; its purpose is to allow the personage that is familiar with this art can understand content of the present invention and is implemented; can not limit protection scope of the present invention with this; all equivalences of doing according to spirit of the present invention change or modify, and all should be encompassed in protection scope of the present invention.
Claims (9)
1. an electronic-grade mixing spent acid reclaims and recycle utilization, it is characterized in that: comprise the following steps of carrying out successively:
(1), analyzes the mass concentration of nitric acid, hydrofluoric acid, silicofluoric acid in the waste liquid;
(2), under stirring condition, add solid sodium salt or sylvite in the waste liquid of step (1), the mol ratio of described sodium salt or sylvite and silicofluoric acid is 0.9 ~ 2:1;
(3), step (2) gained reaction solution is left standstill 0.5 ~ 2h;
(4), the reaction solution after will leaving standstill filters;
(5), the mass concentration of nitric acid, hydrofluoric acid in the reaction solution after the analysis and filter, and interpolation electronic-grade salpeter solution or hydrofluoric acid solution, the mass concentration of nitric acid is adjusted into 15 % ~ 20%, the mass concentration of hydrofluoric acid is adjusted into 5 % ~ 10 %, the mass concentration of silicofluoric acid is adjusted into less than 5 %, then adjusted reaction solution is sent back to production line and uses;
(6), silicofluoride crystal washing that filtration is obtained, behind 100 ~ 150 ℃ of oven dry 2 ~ 3h, obtain the silicofluoride product then.
2. electronic-grade mixing spent acid according to claim 1 reclaims and recycle utilization, it is characterized in that: the mass concentration of nitric acid is that the mass concentration of 5 % ~ 20%, hydrofluoric acid is that the mass concentration of 3% ~ 15 %, silicofluoric acid is 8 % ~ 30 % in the described waste liquid.
3. electronic-grade mixing spent acid according to claim 1 reclaims and recycle utilization, and it is characterized in that: the total acidity of described waste liquid is greater than 50%.
4. electronic-grade mixing spent acid according to claim 1 reclaims and recycle utilization, and it is characterized in that: the metallic cation concentration in the described waste liquid except that sodium ion, potassium ion is less than 1ppm.
5. electronic-grade mixing spent acid according to claim 1 reclaims and recycle utilization, and it is characterized in that: in the step (2), churning time is 1 ~ 3h.
6. electronic-grade mixing spent acid according to claim 1 reclaims and recycle utilization, and it is characterized in that: described sodium salt or sylvite are selected from any in analytically pure saltpetre, SODIUMNITRATE, Potassium monofluoride, Sodium Fluoride, salt of wormwood, the yellow soda ash.
7. electronic-grade mixing spent acid according to claim 1 reclaims and recycle utilization, it is characterized in that: the described sodium salt that 90wt% is above or the salt granularity of sylvite can be passed through 40 mesh sieves.
8. electronic-grade mixing spent acid according to claim 1 reclaims and recycle utilization, it is characterized in that: in the step (4), the reaction solution after leaving standstill is adopted 0.5 micron filter element filtering earlier, then filtrate is adopted 0.01 micron filter element filtering again.
9. electronic-grade mixing spent acid according to claim 1 reclaims and recycle utilization, and it is characterized in that: the purity of described silicofluoride product is greater than 99%.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104591189A (en) * | 2015-02-10 | 2015-05-06 | 湖南有色氟化学科技发展有限公司 | Recycling method for purifying cryolite waste acid |
| CN106395831A (en) * | 2016-08-31 | 2017-02-15 | 池州西恩新材料科技有限公司 | Silicon wafer processing cleaning effluent resource recycling method |
| CN107117753A (en) * | 2016-02-24 | 2017-09-01 | 浙江东氟塑料科技有限公司 | A kind of method that silicon solar cell making herbs into wool devil liquor recovery is utilized |
| CN108046270A (en) * | 2017-12-14 | 2018-05-18 | 江西渠成氟化学有限公司 | A kind of recovery and treatment method of nitration mixture |
| CN111517326A (en) * | 2020-03-27 | 2020-08-11 | 绵阳市鑫科源环保科技有限公司 | Waste acid recovery system and method |
| CN111573951A (en) * | 2020-05-29 | 2020-08-25 | 盛隆资源再生（无锡）有限公司 | Treatment method of semiconductor waste acid |
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| CN102534621A (en) * | 2012-02-21 | 2012-07-04 | 上海正帆科技有限公司 | Method for treating acidic etching solution |
| CN102586780A (en) * | 2012-02-21 | 2012-07-18 | 上海正帆科技有限公司 | Acidic etching solution, as well as preparation method and application thereof |
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2013
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Patent Citations (3)
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| CN102409343A (en) * | 2010-09-24 | 2012-04-11 | 比亚迪股份有限公司 | Regeneration method of waste acid in polysilicon texturing process and waste acid regeneration system |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104591189A (en) * | 2015-02-10 | 2015-05-06 | 湖南有色氟化学科技发展有限公司 | Recycling method for purifying cryolite waste acid |
| CN107117753A (en) * | 2016-02-24 | 2017-09-01 | 浙江东氟塑料科技有限公司 | A kind of method that silicon solar cell making herbs into wool devil liquor recovery is utilized |
| CN106395831A (en) * | 2016-08-31 | 2017-02-15 | 池州西恩新材料科技有限公司 | Silicon wafer processing cleaning effluent resource recycling method |
| CN108046270A (en) * | 2017-12-14 | 2018-05-18 | 江西渠成氟化学有限公司 | A kind of recovery and treatment method of nitration mixture |
| CN111517326A (en) * | 2020-03-27 | 2020-08-11 | 绵阳市鑫科源环保科技有限公司 | Waste acid recovery system and method |
| CN111573951A (en) * | 2020-05-29 | 2020-08-25 | 盛隆资源再生（无锡）有限公司 | Treatment method of semiconductor waste acid |
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| CN103213991B (en) | 2015-09-09 |
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